反应详情

温度

200 °C

Add (R)-4-chloro-5-methyl-5,6-dihydropyrido[2,3-d]pyrimidin-7(8H)-one (0.23 g, 1.18 mmol), 4-(4-isobutyl-1-(2-(pyrrolidin-1-yl)ethyl)-1H-imidazol-2-yl)piperidine trihydrochloride (0.64 g, 1.3 eq), N-methylpyrrolidinone (10 mL) and diisopropylethylamine (1.65 mL, 8.0 eq) in a microwave tube. Seal with crimp cap. Heat in a microwave reactor at 200° C. for 40 minutes. Dilute the reaction mixture with water and extract with ethyl acetate. Wash with saturated aqueous sodium chloride. Dry the organics over anhydrous magnesium sulfate, filter, and concentrate in vacuo. Purify by normal phase chromatography, eluting with hexanes to ethyl acetate to 5% methanol/ethyl acetate to 3% to 5% to 7% to 10% methanol/dichloromethane, to give the title compound (0.13 g, 23%). MS (ES) m/z=466 [M]+.

1. customSeal with crimp cap
2. extractionextract with ethyl acetate
3. washWash with saturated aqueous sodium chloride
4. dry with materialDry the organics over anhydrous magnesium sulfate
5. filtrationfilter
6. concentrationconcentrate in vacuo
7. customPurify by normal phase chromatography
8. washeluting with hexanes to ethyl acetate to 5% methanol/ethyl acetate to 3% to 5% to 7% to 10% methanol/dichloromethane